CN108441912B - Aluminum alloy surface Al3C4-Al2O3-ZrO2The preparation method of wear-resisting composite coating - Google Patents

Aluminum alloy surface Al3C4-Al2O3-ZrO2The preparation method of wear-resisting composite coating Download PDF

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CN108441912B
CN108441912B CN201810217970.5A CN201810217970A CN108441912B CN 108441912 B CN108441912 B CN 108441912B CN 201810217970 A CN201810217970 A CN 201810217970A CN 108441912 B CN108441912 B CN 108441912B
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aluminium alloy
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aluminum alloy
wear
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CN108441912A (en
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黄洁雯
马凌志
樊新民
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Nanjing Tech University
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D9/00Electrolytic coating other than with metals
    • C25D9/04Electrolytic coating other than with metals with inorganic materials
    • C25D9/08Electrolytic coating other than with metals with inorganic materials by cathodic processes
    • C25D9/12Electrolytic coating other than with metals with inorganic materials by cathodic processes on light metals

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Abstract

The invention discloses a kind of aluminum alloy surface Al3C4‑Al2O3‑ZrO2The preparation method of wear-resisting composite coating.For the method using single slot structure electrolytic cell, electrolyte is the mixed solution of zirconium nitrate, urea, formamide and glycerine composition.It in cathode side, is covered using alumina ceramic plate similar with workpiece size, can play non-conductive shielding action in discharge process, reduced because of electric field distortion caused by edge effect around cathode, so that cathodic discharge is more uniform.By applying DC voltage or pulse voltage to electrolytic cell, continuous, uniform air film is quickly formed in cathode surface, continuous plasma micro-arc electric discharge can be caused in aluminum alloy surface, be formed on its surface one layer of stabilization, uniform solid-ceramic coating.The present invention can prepare hardness height, the small wear-and corrosion-resistant coating low with wear rate of coefficient of friction in aluminum alloy surface, effectively widen aluminium alloy in the application in the fields such as traffic, the energy.

Description

Aluminum alloy surface Al3C4-Al2O3-ZrO2The preparation method of wear-resisting composite coating
Technical field
The invention belongs to field of metal surface treatment technology, are related to a kind of aluminum alloy surface Al3C4-Al2O3-ZrO2It is wear-resisting multiple Close the preparation method of coating.
Background technique
Aluminium alloy is widely applied due to having the characteristics that high intensity, high tenacity, light structures, processability are good, being easily recycled In traffic, building materials, Aeronautics and Astronautics etc. be civilian and military industry field, there is irreplaceable weight in national economy and national defense construction It acts on.Since the activity of aluminium alloy itself is higher, surface usually will form the dense oxidation film of layer, although can rise To the effect of certain protection matrix, still, under sliding contact operating condition, mechanism repeatedly makes surface compact oxidation film It peels off, the higher exposed matrix of activity reacts with pair materials such as steel, leads to the adhesive wear of matrix and to secondary material Material transfer, but also coefficient of friction is higher and unstable.In addition, the hardness of aluminium alloy is relatively low, during sliding friction It is easy to happen adhesive wear, thus wearability is relatively poor, seriously limits aluminium alloy in friction system and CONTACT WITH FRICTION component In application.
In order to improve the wear resistance and corrosion resistance of aluminum alloy surface, thermal spraying, physical vapour deposition (PVD), chemical plating or electricity are generallyd use The means such as plating improve aluminium alloy wear-proof corrosion resistance to prepare composite coating.But that there are techniques is cumbersome, at high cost, difficult for these methods In control the disadvantages of, be unfavorable for practical application.Plasma is electrolysed deposition technique (plasma electrolytic It deposition), is one kind directly in the new technology of the alloy surfaces deposition of ceramic coatings such as aluminium, magnesium, titanium.Basic process is will be to Processing workpiece is put into the electrolytic cell for filling specific electrolyte, and is connected with power cathode as cathode, generally use graphite or Platinum is connected as anode with positive pole.After powering on, under electric field action, workpiece surface can occur electrochemistry, heat chemistry, The physical-chemical reaction of a series of complex such as plasma chemistry, ultimately forms ceramic coating.Plasma electrolysis deposition coating Be combined with matrix, the excellent characteristics such as hardness is high, wear-resisting anti-corruption.Document 1 (M.Aliofkhazraei, et al, Carburizing of low-melting-point metals by pulsed nanocrystalline plasma electrolytic carburizing,Surface and Coatings Technology[J],202(2008)5493- 5496.) Al is prepared on 6082 aluminium alloys using cathode plasma electrolytic deposition technology3C4Coating is shown excellent wear-resisting Property.(J.Wu, et al, Anti-corrosion layer prepared by the plasma electrolytic of document 2 carbonitriding on pure aluminum[J], Applied Surface Science,347(2015)673- 678.) composite ceramic coat is prepared on 1060 aluminium alloys using cathode plasma electrolytic deposition technology.Result of study shows The corrosion resistance of composite ceramic coat improves compared with matrix.But it is above-mentioned using cathode plasma electrolytic deposition skill Art prepares composite ceramic coat in aluminum alloy surface and still has average friction coefficient height (0.4~0.5), coating layer thickness too low (2 ~3 μm) the problems such as.
Summary of the invention
The problems such as present invention is low for aluminium and aluminum alloy surface hardness, and coefficient of friction is high and wears no resistance, provides one kind Bond strength height, the aluminum alloy surface Al with excellent wear resistance and corrosion resistance3C4-Al2O3-ZrO2The preparation side of wear-resisting composite coating Method.
The technical scheme is that
Aluminum alloy surface Al3C4-Al2O3-ZrO2The preparation method of wear-resisting composite coating, specific steps are as follows:
Step 1, the pre- aluminium alloy part sand paper for carrying out plasma electric solution deposition is polished smooth, the aluminium alloy leaching after polishing Enter in ethanol solution and is ultrasonically treated, it is dry, obtain pretreated aluminium alloy;
Step 2, aluminum alloy surface side covers and is placed in cathode using alumina ceramic plate, in aluminium alloy and potsherd A circular hole is made a call on top, is fixed by double nut or so cooperation, so that workpiece is combined closely with potsherd;
Step 3, the spacing of cathode and anode is controlled in 60~80mm, area ratio control carries out aluminium alloy 6~8 Cathode plasma electrolysis processing, using urea-glycerine system as electrolyte, setting voltage is 150~160V, will apply voltage liter To 180V~200V, the retention time, 40~55%, frequency was controlled in 50Hz~400Hz for duty ratio control in 10~15min, In the electrolyte, the concentration of urea is 300~350g/L, and the concentration of formamide is 180~200g/L, the concentration of glycerine For 100~150g/L, the concentration of zirconium nitrate is 15~20g/L, and the concentration of ammonium nitrate is 3~5g/L, and the concentration of potassium chloride is 10 ~20g/L.
Preferably, in step 1, the ultrasonic time is 10~15min.
Preferably, in step 2, the diameter of the circular hole is 3~4mm.
Preferably, in step 3, the rate of pressure rise is 5~7V/min.
In cathode plasma electrolytic process, alumina ceramic plate can produce in plasma electrolyting precipitation process as Lower effect: (1) during plasma discharge, plasma temperature is up to 3000 DEG C, easily by aluminum alloy melting, and uses oxygen Changing aluminium potsherd can reduce plasma discharge area, reduces cathode self-temperature, aluminium alloy is prevented to be melted;(2) by In the nonconducting characteristic of alumina ceramic plate itself, non-conductive shielding action is played between two electrodes, can be reduced around cathode Because of electric field distortion caused by edge effect, so that cathodic discharge is more uniform.
Compared with prior art, the invention has the following advantages that
(1) coating is deposited directly to metal surface, good with substrate combinating strength, can locate after aluminium alloy polishing cleaning Reason, electroless plating, the cumbersome pretreatment such as chemical plating.
(2) plasma electrodeposition process electrolyte that is simple, high-efficient, not limited by workpiece shapes, and used Pollute small, at low cost, favorable repeatability.
(3) after adding zirconium oxide in the coating, the corrosion resistance of coating is significantly improved, compared with matrix, electric current Density reduces nearly two orders of magnitude.Also, since the zirconia particles of coating surface play the role of lubrication antifriction, friction system Number is reduced to 0.18 or so, has low wear rate (0.021mm3/ Nm) and good corrosion resisting property (corrosion electric current density 8.82 ×10-6A/cm2), wear rate has dropped 93.3% compared with matrix.
(4) cathode back is covered in using alumina ceramic plate, plays non-conductive shielding action, can reduces around cathode Because of electric field distortion caused by edge effect, so that cathodic discharge is more uniform.
Detailed description of the invention
Fig. 1 is is used electrolyser construction schematic diagram.
Fig. 2 is the coefficient of friction schematic diagram that composite coating is prepared under different electrolytes.
Fig. 3 is the polarization curve schematic diagram that composite coating is prepared under different electrolytes.
Specific embodiment
The invention will be further described with reference to the accompanying drawings and examples.
Embodiment 1
(1) using electrolyser construction shown in Fig. 1, by the pre- aluminium alloy part sand paper polishing light for carrying out plasma electric solution deposition It is sliding, the aluminium alloy after polishing is immersed in ethanol solution and is ultrasonically treated, it is dry, obtain pretreated aluminium alloy;
(2) aluminum alloy surface side covers and is placed in cathode using alumina ceramic plate, on aluminium alloy and potsherd A circular hole is made a call in portion, is fixed by double nut or so cooperation, so that workpiece is combined closely with potsherd.By cathode and anode Spacing control is controlled in 70mm, area ratio 7;
(3) use urea-glycerine system for electrolyte, the concentration of urea is 325g/L, and the concentration of formamide is 190g/L, the concentration of glycerine are 125g/L, and the concentration of zirconium nitrate is 17g/L, and the concentration of ammonium nitrate is 4g/L, potassium chloride it is dense Degree is 15g/L;
(4) cathode plasma electrolysis processing is carried out to aluminium alloy, applied voltage is 155V, later with the rate of 6V/min Voltage will be applied and rise to 190V.Retention time is in 12min.50%, frequency is controlled in 250Hz for duty ratio control.Make when reaction With water-cooled process, solution temperature is at 40 DEG C or so when making to react;
The thickness of composite coating is measured at 60 μm.Under the load of 6N, using silicon carbide steel ball as abrasive material, tried in friction Progress 30min reciprocating friction wear test on machine is tested, measuring average friction coefficient is 0.21, wear rate 0.034mm3/ Nm.Electronic bit polarization curve test is carried out in 3.5%NaCl solution, corrosion current is 5.82 × 10-6A/cm2
Embodiment 2
(1) using electrolyser construction shown in Fig. 1, by the pre- aluminium alloy part sand paper polishing light for carrying out plasma electric solution deposition It is sliding, the aluminium alloy after polishing is immersed in ethanol solution and is ultrasonically treated, it is dry, obtain pretreated aluminium alloy;
(2) aluminum alloy surface side covers and is placed in cathode using alumina ceramic plate, on aluminium alloy and potsherd A circular hole is made a call in portion, is fixed by double nut or so cooperation, so that workpiece is combined closely with potsherd.By cathode and anode Spacing control is controlled in 60mm, area ratio 6;
(3) use urea-glycerine system for electrolyte, the concentration of urea is 300g/L, and the concentration of formamide is 180g/L, the concentration of glycerine are 100g/L, and the concentration of zirconium nitrate is 15g/L, and the concentration of ammonium nitrate is 3g/L, potassium chloride it is dense Degree is 10g/L;
(4) cathode plasma electrolysis processing is carried out to aluminium alloy, applied voltage is 150V, later with the rate of 5V/min Voltage will be applied and rise to 180V.Retention time is in 10min.40%, frequency is controlled in 50Hz for duty ratio control.It is used when reaction Water-cooled process, solution temperature is at 40 DEG C or so when making to react;
The thickness of composite coating is measured at 45 μm.Under the load of 6N, using silicon carbide steel ball as abrasive material, tried in friction Progress 30min reciprocating friction wear test on machine is tested, measuring average friction coefficient is 0.26, wear rate 0.039mm3/ Nm.Electronic bit polarization curve test is carried out in 3.5%NaCl solution, corrosion current is 4.38 × 10-6A/cm2
Embodiment 3
(1) using electrolyser construction shown in Fig. 1, by the pre- aluminium alloy part sand paper polishing light for carrying out plasma electric solution deposition It is sliding, the aluminium alloy after polishing is immersed in ethanol solution and is ultrasonically treated, it is dry, obtain pretreated aluminium alloy;
(2) aluminum alloy surface side covers and is placed in cathode using alumina ceramic plate, on aluminium alloy and potsherd A circular hole is made a call in portion, is fixed by double nut or so cooperation, so that workpiece is combined closely with potsherd.By cathode and anode Spacing control is controlled in 80mm, area ratio 8;
(3) use urea-glycerine system for electrolyte, the concentration of urea is 350g/L, and the concentration of formamide is 200g/L, the concentration of glycerine are 150g/L, and the concentration of zirconium nitrate is 20g/L, and the concentration of ammonium nitrate is 5g/L, potassium chloride it is dense Degree is 20g/L.
(4) cathode plasma electrolysis processing is carried out to aluminium alloy, applied voltage is 160V, later with the rate of 7V/min Voltage will be applied and rise to 200V.Retention time is in 15min.55%, frequency is controlled in 400Hz for duty ratio control.Make when reaction With water-cooled process, solution temperature is at 40 DEG C or so when making to react.
The thickness of composite coating is measured at 70 μm.Under the load of 6N, using silicon carbide steel ball as abrasive material, tried in friction Progress 30min reciprocating friction wear test on machine is tested, measuring average friction coefficient is 0.18, wear rate 0.021mm3/ Nm.Electronic bit polarization curve test is carried out in 3.5%NaCl solution, corrosion current is 8.82 × 10-6A/cm2
Comparative example 1
This comparative example and embodiment 1 are essentially the same, unique the difference is that without addition zirconium nitrate and nitre in the electrolyte Sour ammonium.
The thickness of composite coating is measured at 60 μm.Under the load of 6N, using silicon carbide steel ball as abrasive material, tried in friction The reciprocating friction wear test carried out 30 minutes is tested on machine, and measuring average friction coefficient is 0.34, and wear rate is 0.028mm3/Nm.Electronic bit polarization curve test is carried out in 3.5%NaCl solution, corrosion current is 4.42 × 10-5A/ cm2
In Fig. 2, a is the coefficient of friction signal for being added to the composite coating of zirconium nitrate and ammonium nitrate preparation in the electrolytic solution Figure, b are the coefficient of friction schematic diagram for being not added with the composite coating of zirconium nitrate and ammonium nitrate preparation in the electrolytic solution.Coating a's rubs Coefficient average out to 0.18 is wiped, the coefficient of friction average out to 0.34 of coating b is apparently higher than coating a.
In Fig. 3, a is the polarization curve signal for being added to the composite coating of zirconium nitrate and ammonium nitrate preparation in the electrolytic solution Figure, b are the polarization curve schematic diagram for being not added with the composite coating of zirconium nitrate and ammonium nitrate preparation in the electrolytic solution.The corruption of coating a Erosion current density improves 1 order of magnitude compared with coating b.
Comparative example 2
This comparative example and embodiment 1 are essentially the same, unique the difference is that without addition ammonium nitrate in the electrolyte.
In plasma electrolyting precipitation process, since zirconium nitrate forms zirconium hydroxide gel, cause cathode surface cannot Regular picture.Therefore, ceramic coating can not be prepared on aluminium alloy using this electrolyte.
Comparative example 3
This comparative example and embodiment 1 are essentially the same, unique the difference is that the additive amount of ammonium nitrate is in the electrolyte 15g。
In plasma electrolyting precipitation process, since the additive amount of inorganic salts in electrolyte is excessive so that cathode surface air film Electric current when breakdown is excessive, and aluminium alloy is caused to dissolve because temperature is excessive.It therefore, can not be in aluminium alloy table using this electrolyte Ceramic coating is prepared on face.
Comparative example 4
This comparative example and embodiment 1 are essentially the same, unique the difference is that the additive amount of zirconium nitrate is in the electrolyte 30g。
In plasma electrolyting precipitation process, since ammonium nitrate additive amount is limited in electrolyte, zirconium hydroxide can not be inhibited Formation cause solution formed gel, prevent cathode surface is from regular picture.Therefore, it can not be closed in aluminium using this electrolyte Ceramic coating is prepared in gold surface.

Claims (4)

1. aluminum alloy surface Al3C4-Al2O3-ZrO2The preparation method of wear-resisting composite coating, which is characterized in that specific steps are as follows:
Step 1, the pre- aluminium alloy part sand paper for carrying out plasma electric solution deposition is polished smooth, the aluminium alloy after polishing immerses second It is ultrasonically treated in alcoholic solution, it is dry, obtain pretreated aluminium alloy;
Step 2, aluminum alloy surface side covers and is placed in cathode using alumina ceramic plate, in aluminium alloy and potsherd top A circular hole is made a call to, is fixed by double nut or so cooperation, so that workpiece is combined closely with potsherd;
Step 3, the spacing of cathode and anode is controlled in 60~80mm, area ratio control carries out cathode 6~8, to aluminium alloy Plasma electrolysis processing, using urea-glycerine system as electrolyte, setting voltage is 150~160V, will apply voltage and rises to 180V~200V, the retention time, 40~55%, frequency was controlled in 50Hz~400Hz, institute for duty ratio control in 10~15min In the electrolyte stated, the concentration of urea is 300~350g/L, and the concentration of formamide is 180~200g/L, and the concentration of glycerine is 100~150g/L, the concentration of zirconium nitrate are 15~20g/L, and the concentration of ammonium nitrate is 3~5g/L, the concentration of potassium chloride is 10~ 20g/L。
2. preparation method according to claim 1, which is characterized in that in step 1, the ultrasonic time be 10~ 15min。
3. preparation method according to claim 1, which is characterized in that in step 2, the diameter of the circular hole is 3~ 4mm。
4. preparation method according to claim 1, which is characterized in that in step 3, the voltage that will apply rises to 180V Rate of pressure rise when~200V is 5~7V/min.
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CN111676499A (en) * 2020-07-30 2020-09-18 华南理工大学 Hydrogen-resistant coating based on cathode plasma electrolytic deposition and preparation method thereof
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